反応 #43305

反応方程式

4-amino-3-mercapto-5-(3,4,5-trimethoxyphenyl)-4H-1,2,4-triazole

3H-benzo[d]imidazole-5-carboxylic acid

→

title compound

収率 17.5%

6-(1H-Benzo[d]imidazol-6-yl)-3-(3,4,5-trimethoxyphenyl)-[1,2,4]triazolo[3,4-b][1,3,4]thiadiazole

収率 17.5%

溶媒

phosphoryl chloride

反応条件

後処理

1. 1
   温度was refluxed for 3 h
2. 2
   その他The solvent was evaporated
3. 3
   workup.DISSOLUTIONthe residue was dissolved in dichloromethane (20 mL)
4. 4
   乾燥The organic layer was dried over sodium sulfate
5. 5
   濃縮concentrated

実験手順

A mixture of 4-amino-3-mercapto-5-(3,4,5-trimethoxyphenyl)-4H-1,2,4-triazole (80 mg, 0.28 mmol) and 3H-benzo[d]imidazole-5-carboxylic acid (46 mg, 0.28 mmol) in phosphoryl chloride (2 mL) was refluxed for 3 h. The solvent was evaporated and the residue was dissolved in dichloromethane (20 mL). It was neutralized with aqueous sodium carbonate. The organic layer was dried over sodium sulfate, concentrated to give 20 mg (17%) of the title compound as a solid. 1H NMR (CD3OD): 8.55 (s, 1H), 8.35 (s, 1H), 8.01-7.85 (m, 2H), 7.72 (s, 1H), 3.99 (s, 6H), 3.87 (s, 3H).

出典